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Polymeric intumescent coatings are fire protective materials that increase their thermal resistance when exposed to high temperatures to prevent building structures from damage. The idea of the investigation was to develop a simple test method to determine the time dependent thermal conductivity of intumescent coatings. Therefore steel plates were coated with two different intumescent systems. During cone calorimeter tests the temperature at the back side of the coated plates was measured. These results were used to calculate the time dependent thermal resistance of the protective layer with the simulation program IOPT2D for different external heat fluxes and different layer thickness.
Polymeric nanocomposites are discussed as one of the most promising advanced materials whose nanoscale effects can be exploited for industry. Layered silicate polypropylene-graft-maleic anhydride nanocomposites are investigated as a model to clarify the potential of such materials in terms of fire retardancy. The nanostructure is characterized using transmission electron microscopy (TEM) and shear viscosity. The fire behavior is characterized using different external heat fluxes in cone calorimeter, limiting oxygen index and UL 94 classification. A comprehensive fire behavior characterization is presented which enables an assessment of the materials’ potential with respect to different fire scenarios and fire tests. The influence of morphology and the active mechanisms are discussed, such as barrier formation and changed melt viscosity. To our knowledge, it is the first attempt to illuminate the concept’s strengths, such as the reduction of flame spread, and weaknesses, such as the lack of influence on ignitability, in a clear, comprehensive and detailed manner.
The influence of different organobentonites on the decomposition and the combustion behaviour of an epoxy resin were examined. The epoxy resin is a cationically polymerised cycloaliphatic epoxy resin flexibilised with poly(tetrahydrofuran) (PTHF), with hydroxyl endgroups. The bentonite was modified with either an ammonium or a phosphonium salt. The thermal decomposition of the PTHF induced by the initiator, used for the cationic polymerisation, did neither take place for the nanocomposite based on the ammonium bentonite nor for that based on the phosphonium bentonite. This improved decomposition characteristic lead to a larger time to ignition for both kinds of nanocomposites compared to the not modified polymer, which is not the case for other polymer/clay nanocomposites described in the literature. The fire behaviour was investigated using limiting oxygen index (LOI), a horizontal burner test and a cone calorimeter. The forced flaming conditions in the cone calorimeter were varied using different external heat fluxes between 30 and 70 kW · m-2. The fire behaviour of the nanocomposites was improved in comparison to the polymer, and phosphonium bentonite was superior to ammonium bentonite. The main mechanism is a barrier formation resulting in a reduction of the fire growth rate, which was more pronounced in the case of high external heat fluxes.
A method was developed to assess the heat insulation performance of intumescent coatings. The method consists of temperature measurements using the bench-scaled experimental set-up of a cone calorimeter and finite difference simulation to calculate the effective thermal conductivity dependent on time/temperature. This simulation procedure was also adapted to the small scale test furnace, in which the standard time-temperature curve is applied to a larger sample and thus which provides results relevant for approval. Investigations on temperature and calculated effective thermal conduction were performed on intumescent coatings in both experimental set-ups using various coating thicknesses. The results correspond to each other as well as showing the limits of transferability between both fire tests. It is shown that bench-scaled cone calorimeter tests are a valuable tool for assessing and predicting the performance of intumescent coatings in larger tests relevant for approval. The correlation fails for processes at surface temperatures above 750°C, which are not reached in the cone calorimeter, but are attained in the small scale furnace set-up.
The cone calorimeter has become one of the most important and widely used instruments for the research and development of fire retarded polymeric materials. The paper addresses three important ways in which the principal setup influences the results factors which sometimes do not receive due consideration when drawing conclusions. The paper discusses in detail the impact on cone calorimeter results of the choice of external heat flux, the influence on the peak of heat release rate of sample thickness and thermal feedback from the back of the sample, and the influence on irradiance of the horizontal and vertical distances from the cone heater.
Barrier formation and increasing the melt viscosity are addressed as the two main general fire retardancy mechanisms of polymer nanocomposites. They result in specific impacts on fire properties that consequentially cause varying flame retardancy efficiency in different fire tests. The barrier formation retards mainly flame spread (peak of heat release rate) in developing fires, but does not reduce fire load (total heat evolved), ignitability or flammability (limiting oxygen index, UL 94). Furthermore, this flame retardancy effect increases with increasing irradiation and vanishes with decreasing irradiation. The increased melt viscosity prevents dripping, which is beneficial or disadvantageous depending on the fire test used. In some test, it become the dominant influence, transforming self-extinguishing samples into flammable materials or causing wicking. Advantages and the limits are sketched comprehensively for exploiting the main general fire retardancy mechanisms of polymer nanocomposites. It is concluded that barrier formation and changing the melt viscosity in nanocomposites are not sufficient for most applications, but must be accompanied by additional mechanisms in special systems or in combination with other flame retardants.
Thermogravimetry (TG), thermogravimetry coupled with mass spectroscopy (TG-MS) and thermogravimetry coupled with Fourier transform infrared spectroscopy (TG-FTIR) were used to characterise the thermo-oxidative behaviour of two intumescent coating materials. The temperature dependence, the corresponding volatile products and the amount of residue of the different processes were determined. Using both TG-MS and TG-FTIR results in an unambiguous interpretation of the volatile products. Characteristics such as the influence of endothermic reactions, the release of non-flammable gases, the dehydrogenation enhancing the char formation and the stability of the cellular char were discussed in detail. It was demonstrated, that TG, TG-MS and TG-FTIR are powerful methods to investigate mechanisms in intumescent coatings and that they are suitable methods in respect to quality assurance and unambiguous identification of such materials.
The exploration of condensed phase mechanisms such as charring and intumescence has been pushed forward in the last decades, since it is believed that focusing on these concepts will bring materials closer to an efficient and ecologically friendly fire retardancy. They promise to concentrate efficient fire retardancy at the key position between pyrolysis zone and gas phase. Examples of residue/char forming and intumescent materials are used to illustrate the influence of mass and heat barrier effects on the fire behavior of materials and general results are presented. A comprehensive understanding of the mechanisms and structure-property relationships in fire retardancy is presented.
Nanocomposites of bisphenol A polycarbonate with 2, 4, 6, and 15 wt% multiwall carbon nanotubes (MWNT) and their use in fire retardancy are investigated. Their thermal behavior and pyrolysis are characterized using thermogravimetry, differential scanning calorimeter, oscillatory shear rheology, and dynamic mechanical analysis. The flammability is addressed using LOI and UL 94; the fire behavior, with a cone calorimeter using different irradiation. With increasing MWNT content the storage modulus is increased (10-20%) and melt viscosity increases by several orders of magnitude, particularly for low shear rates. The melt flow, dripping, and deformation during fire are hindered, which influences UL 94 and cone calorimeter results. The peak heat release rate is reduced up to 40-50% due to an improved barrier for small amounts (2 wt%) of MWNT and for low irradiation, whereas the effect is reduced for increasing irradiation and nearly vanishes for increasing filling. Adjuvant but also deleterious mechanisms result in the complex dependency on the MWNT content. Significant flame retardancy effects are specific and limited to only some fire properties. This study allows the materials' potential for implementation in different fire scenarios and tests to be assessed and provides insight into active mechanisms.